Determination of Cholesterol in Aquatic Products by UHPLC after Hydrolysis with Alkaline Ionic Liquid and Extraction with Aqueous Two-Phase Micellar System
摘 要
基于碱性离子液体水解以及双水相胶束体系(ATPMS)提取,以超高效液相色谱法(UHPLC)测定水产品中胆固醇的含量,并以分配系数为指标对ATPMS组成进行了优化。称取0.10 g肉糜状水产品,加入0.36 mol·L-1氢氧化1-丁基-3-甲基咪唑盐([C4mim]OH)碱性离子液体1 mL,于90℃加热30 min,冷却后以5 000 r·min-1转速离心5 min。取全部上清液,加入3 mL由0.5%(质量分数,下同)1-丁基-3-甲基咪唑乙酸盐[C4mim]Ac离子液体和5.0%(质量分数,下同) Triton X-114组成的ATPMS[介质为柠檬酸-磷酸盐缓冲液(pH 7.0)],加热至浊点,保持3 min,取出下层相,用甲醇定容至5 mL,涡旋30 s,超声5 min。分取1 mL过0.22 μm滤膜,滤液供UHPLC分析。结果显示:以由0.5% 1-丁基-3-甲基咪唑咪唑盐([C4mim]Im)或[C4mim]Ac和5.0% Triton X-114组成的ATPMS提取胆固醇时,所得分配系数较高;胆固醇的质量浓度在5~200 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为7.5 μg·g-1;由[C4mim]Ac组成的ATPMS所得的回收率(84.1%~89.9%)略大于由[C4mim]Im组成的ATPMS的(80.0%~83.9%),且和参考GB 5009.128-2016设置的对照组(催化剂为氢氧化钾,提取剂为甲醇)的接近,3组试验测定值的相对标准偏差(n=5)基本一致,均小于3.0%。
Abstract
Method for determination of cholesterol in aquatic products was proposed by UHPLC based on alkaline ionic liquid hydrolysis and aqueous two-phase micellar system (ATPMS) extraction, and the composition of ATPMS was optimised in terms of partition coefficient. Minced meat packed aquatic product of 0.10 g was taken and mixed with 0.36 mol·L-1 hydroxide 1-butyl-3-methylimidazole salt ([C4mim]OH) alkaline ionic liquid (1 mL), and the mixture was heated at 90 ℃ for 30 min. After cooling and centrifuging at 5 000 r·min-1 for 5 min, the entire supernatant was taken, 3 mL of ATPMS [citric acid-phosphate buffer (pH 7.0) as media] consisting of 0.5% (mass fraction, the same below) 1-butyl-3-methyl imidazole acetate ([C4mim]Ac) and 5.0% (mass fraction, the same below) Triton X-114 was added, and the mixture was heated to the cloud point, keeping for 3 min. The lower phase was taken, diluted to 5 mL with methanol, vortexed for 30 s and sonicated for 5 min. An aliquot (1 mL) of the above solution was taken and passed through 0.22 μm filter membrane and the filtrate was used for UHPLC analysis. It was shown by results that the ATPMS consisting of 0.5% [C4mim]Im or [C4mim]Ac and 5.0% Triton X-114 gave a high partition coefficient for extraction of cholesterol. Linear relationship between the mass concentration of cholesterol and respective peak area was kept in the range of 5-200 mg·L-1, with detection limit (3S/N) of 7.5 μg·g-1; the results (84.1%-89.9%) of recovery obtained from the ATPMS containing [C4mim]Ac were slightly higher than those (80.0%-83.9%) obtained from the ATPMS containing [C4mim]Im, and were similar to those obtained from the control group with reference to GB 5009.128-2016 (KOH as catalyst and methanol as extractant). RSDs (n=5) of the determined values of the three groups were basically the same and less than 3.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202202005
所属栏目 工作简报
基金项目 浙江省分析测试科技计划项目(2018C37023)
收稿日期 2020/7/13
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备注宋玉凤,硕士研究生,主要研究方向为水产品的质量与安全
引用该论文: SONG Yufeng,ZHU Junxiang,YU Dingyi,ZHANG Xiaojun,MA Jianfeng. Determination of Cholesterol in Aquatic Products by UHPLC after Hydrolysis with Alkaline Ionic Liquid and Extraction with Aqueous Two-Phase Micellar System[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(2): 152~156
宋玉凤,朱俊向,于丁一,张小军,马剑锋. 碱性离子液体水解-双水相胶束体系提取-超高效液相色谱法测定水产品中胆固醇的含量[J]. 理化检验-化学分册, 2022, 58(2): 152~156
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参考文献
【1】LECERF J M, DE LORGERIL M. Dietary cholesterol:From physiology to cardiovascular risk[J]. The British Journal of Nutrition, 2011,106(1):6-14.
【2】BARTER P, GOTTO A M, LAROSA J C, et al. HDL cholesterol, very low levels of LDL cholesterol, and cardiovascular events[J]. New England Journal of Medicine, 2007,357(13):1301-1310.
【3】谭观岳,傅红,杨琳.HPLC和试剂盒两种测定鳗鱼胆固醇方法的比较[J].食品研究与开发, 2008,29(4):148-150.
【4】王潇,穆迎春,朱俊向.超高效液相色谱法测定中华绒螯蟹的胆固醇含量[J].分析仪器, 2019(1):125-128.
【5】齐东健,时维平.气相色谱法测定水产品中的胆固醇[J].海峡预防医学杂志, 2002,8(3):56-57.
【6】丁磊,胡艳云,韩芳,等.固相萃取-液相色谱-串联质谱法测定动植物油脂中胆固醇[J].理化检验-化学分册, 2018,54(5):596-600.
【7】CLAUSEN D N, VISENTAINER J V, TARLEY C R. Development of molecularly imprinted poly(methacrylic acid)/silica for clean-up and selective extraction of cholesterol in milk prior to analysis by HPLC-UV[J]. The Analyst, 2014,139(19):5021-5027.
【8】ALBUQUERQUE T G, OLIVEIRA M B, SANCHES-SILVA A, et al. Cholesterol determination in foods:Comparison between high performance and ultra-high performance liquid chromatography[J]. Food Chemistry, 2016,193:18-25.
【9】MOLINO J V, MARQUES D A, JUNIOR A P, et al. Different types of aqueous two-phase systems for biomolecule and bioparticle extraction and purification[J]. Biotechnology Progress, 2013,29(6):1343-1353.
【10】MUKHERJEE P, PADHAN S K, DASH S, et al. Clouding behaviour in surfactant systems[J]. Advances in Colloid and Interface Science, 2011,162(1/2):59-79.
【11】VICENTE F A, MALPIEDI L P, E SILVA F A, et al. Design of novel aqueous micellar two-phase systems using ionic liquids as co-surfactants for the selective extraction of (bio)molecules[J]. Separation and Purification Technology, 2014,135:259-267.
【12】TORRES F A E, DE ALMEIDA FRANCISCO A C, PEREIRA J F B, et al. Imidazolium-based ionic liquids as co-surfactants in aqueous micellar two-phase systems composed of nonionic surfactants and their aptitude for recovery of natural colorants from fermented broth[J]. Separation and Purification Technology, 2018,196:262-269.
【13】ISHAK Z I, SAIRI N A, ALIAS Y, et al. A review of ionic liquids as catalysts for transesterification reactions of biodiesel and glycerol carbonate production[J]. Catalysis Reviews, 2017,59(1):44-93.
【14】CHEN F L, ZHANG X L, ZHANG Q, et al. Simultaneous synergistic microwave-ultrasonic extraction and hydrolysis for preparation of trans-resveratrol in tree peony seed oil-extracted residues using imidazolium-based ionic liquid[J]. Industrial Crops and Products, 2016,94:266-280.
【2】BARTER P, GOTTO A M, LAROSA J C, et al. HDL cholesterol, very low levels of LDL cholesterol, and cardiovascular events[J]. New England Journal of Medicine, 2007,357(13):1301-1310.
【3】谭观岳,傅红,杨琳.HPLC和试剂盒两种测定鳗鱼胆固醇方法的比较[J].食品研究与开发, 2008,29(4):148-150.
【4】王潇,穆迎春,朱俊向.超高效液相色谱法测定中华绒螯蟹的胆固醇含量[J].分析仪器, 2019(1):125-128.
【5】齐东健,时维平.气相色谱法测定水产品中的胆固醇[J].海峡预防医学杂志, 2002,8(3):56-57.
【6】丁磊,胡艳云,韩芳,等.固相萃取-液相色谱-串联质谱法测定动植物油脂中胆固醇[J].理化检验-化学分册, 2018,54(5):596-600.
【7】CLAUSEN D N, VISENTAINER J V, TARLEY C R. Development of molecularly imprinted poly(methacrylic acid)/silica for clean-up and selective extraction of cholesterol in milk prior to analysis by HPLC-UV[J]. The Analyst, 2014,139(19):5021-5027.
【8】ALBUQUERQUE T G, OLIVEIRA M B, SANCHES-SILVA A, et al. Cholesterol determination in foods:Comparison between high performance and ultra-high performance liquid chromatography[J]. Food Chemistry, 2016,193:18-25.
【9】MOLINO J V, MARQUES D A, JUNIOR A P, et al. Different types of aqueous two-phase systems for biomolecule and bioparticle extraction and purification[J]. Biotechnology Progress, 2013,29(6):1343-1353.
【10】MUKHERJEE P, PADHAN S K, DASH S, et al. Clouding behaviour in surfactant systems[J]. Advances in Colloid and Interface Science, 2011,162(1/2):59-79.
【11】VICENTE F A, MALPIEDI L P, E SILVA F A, et al. Design of novel aqueous micellar two-phase systems using ionic liquids as co-surfactants for the selective extraction of (bio)molecules[J]. Separation and Purification Technology, 2014,135:259-267.
【12】TORRES F A E, DE ALMEIDA FRANCISCO A C, PEREIRA J F B, et al. Imidazolium-based ionic liquids as co-surfactants in aqueous micellar two-phase systems composed of nonionic surfactants and their aptitude for recovery of natural colorants from fermented broth[J]. Separation and Purification Technology, 2018,196:262-269.
【13】ISHAK Z I, SAIRI N A, ALIAS Y, et al. A review of ionic liquids as catalysts for transesterification reactions of biodiesel and glycerol carbonate production[J]. Catalysis Reviews, 2017,59(1):44-93.
【14】CHEN F L, ZHANG X L, ZHANG Q, et al. Simultaneous synergistic microwave-ultrasonic extraction and hydrolysis for preparation of trans-resveratrol in tree peony seed oil-extracted residues using imidazolium-based ionic liquid[J]. Industrial Crops and Products, 2016,94:266-280.
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